CN106753237B - A kind of graphene/ferroso-ferric oxide composite wave-suction material and preparation method thereof - Google Patents
A kind of graphene/ferroso-ferric oxide composite wave-suction material and preparation method thereof Download PDFInfo
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Abstract
The present invention is suitable for absorbing material field, provides a kind of graphene/ferroso-ferric oxide composite wave-suction material and preparation method thereof.The preparation method comprises the following steps: preparation graphene oxide dispersion, FeCl2Solution and FeCl3Solution；Above-mentioned three kinds of liquid is mixed, is stirred 2-3 hours under 80-120 degree, graphene oxide/Fe is obtained3O4Dispersion liquid；By the graphene oxide/Fe3O4Dispersion liquid vacuum drying, obtains graphene oxide/Fe3O4Aeroge；By the graphene oxide/Fe3O4Aeroge heating, obtains graphene/Fe3O4Aeroge, by the graphene/Fe3O4Aeroge carries out Mechanical pressing, obtains graphene/Fe3O4Composite material；Graphene/the Fe3O4Composite material is the layer structure that lamella stacks.Graphene/Fe provided by the invention3O4Composite wave-suction material electromagnetic performance matching feature make its more absorb rather than reflection electromagnetic wave, to reduce secondary pollution of the electromagnetic wave to environment.
Description
Technical field
The invention belongs to absorbing material field more particularly to a kind of graphene/ferroso-ferric oxide composite wave-suction material and its
Preparation method.
Background technique
Absorbing material, which refers to, can absorb the electromagnetic wave energy for projecting its surface, and by the dielectric loss of material by electromagnetism
Wave energy is converted to the material of the energy of thermal energy or other forms.As the rapid development and people of modern science and technology technology are to strong
The continuous improvement of health quality requirement, the research and development of new and effective absorbing material are by extensive concern.
Graphene is a kind of two-dimensional material of only single carbon atom thickness, and graphene not only has excellent mechanics, heat
And electric property, but also there are good Microwave Absorption Properties.The lamellar structure of graphene is conducive to improve multiple reflections
Loss, the high conductivity of graphene advantageously form good conductive network, achieve the effect that electro-magnetic wave absorption, especially in X wave
Duan Xiaoguo becomes apparent, and the graphene of two-dimensional slice structure has advantageous advantage in absorbing material field.Ferrite is inhaled
Wave material is iron-series metal oxide or composite oxides, belongs to ferrimagnetic material.Its absorbing property from ferromagnetism and
Dielectric properties, relative permeability and relative dielectric constant are in plural form, can generate dielectric loss but also generate magnetic loss
Consumption, therefore there is good absorbing property.Simultaneously because its resistivity is higher, electromagnetic wave easily enters and rapid decay, can make
It is still able to maintain high magnetic conductivity in high frequency.It is usually that its is compound next but due to the deficiencies of its density is big, and hot properties is poor
Obtain good absorbing material.
In graphene/ferriferrous oxide composite material of traditional method preparation, ferroferric oxide magnetic nanoparticle is difficult
It is fully dispersed to be obtained in graphene oxide substrate；And during restoring, due to the addition of the reducing agents such as hydrazine hydrate, not only
With toxicity, and environment is polluted, the recovery time is long, waste of energy；The graphene of preparation/ferriferrous oxide composite material conductance
Rate is low, to affect wave-absorbing effect.In addition, graphene/ferriferrous oxide composite material of conventional method preparation is usually powder
Last structure, density are big, it is difficult to form a film, absorption band is narrow, and absorbing property is poor.
Therefore, the prior art could be improved.
Summary of the invention
In order to solve the above technical problems, the present invention provides a kind of graphene/ferroso-ferric oxide composite wave-suction material and its system
Preparation Method, it is intended to improve existing graphene/Fe3O4The performance of composite material.
The invention is realized in this way a kind of graphene/ferroso-ferric oxide composite wave-suction material preparation method, including with
Lower step:
Prepare graphene oxide dispersion, FeCl2Solution and FeCl3Solution；
Above-mentioned three kinds of liquid is mixed, is stirred in 80-120 degree, graphene oxide/Fe is obtained3O4Dispersion liquid；
By the graphene oxide/Fe3O4Dispersion liquid vacuum drying, obtains graphene oxide/Fe3O4Aeroge；
By the graphene oxide/Fe3O4Aeroge heating, obtains graphene/Fe3O4Aeroge, by the graphene/
Fe3O4Aeroge carries out Mechanical pressing, obtains graphene/Fe3O4Composite material；Graphene/the Fe3O4Composite material is lamella
The layer structure of stacking.
Further, the preparation process of the graphene oxide dispersion includes: that graphene oxide is soluble in water, ultrasound
Handle 30-40min；The concentration of the graphene oxide dispersion is 0.1-10mg/ml, FeCl2The concentration of solution is 10-
20mg/ml, FeCl3The concentration of solution is 20-30mg/ml.
Further, the graphene oxide dispersion, FeCl2Solution and FeCl3The volume ratio of solution is 5-10:1-3:
2-4。
Further, the graphene oxide/Fe3O4Fe in dispersion liquid3O4Content is 10-50%, the Fe3O4Grain
Diameter is 20-60nm.
Further, the vacuum drying temperature is 60-80 degree, time 18-24h.
Further, the heating temperature is 200-400 DEG C, and the time is 2-4 hours.
Further, the graphene/Fe3O4The density of aeroge is 0.1-1g/cm3。
Further, the graphene/Fe3O4Composite material with a thickness of 0.01-5nm.
Further, the graphene/Fe3O4Composite material with a thickness of 1-2 μm, suction wave efficiency be 25-62dB.
The present invention also provides a kind of graphene/ferroso-ferric oxide composite wave-suction materials, using above-mentioned preparation method system
At.
Compared with prior art, the present invention beneficial effect is: graphene/ferroso-ferric oxide provided in an embodiment of the present invention
The preparation method of composite wave-suction material makes full use of rich in-OH in graphene oxide, and the functional groups such as-COOH can be used as nucleation
Site reacts with iron ion and ferrous ion and generates Fe3O4.The preparation method first uses graphene oxide dispersion, FeCl2
Solution and FeCl3Solution prepares graphene oxide/Fe3O4Aeroge, Fe3O4Surface and piece of the uniform load in graphene carrier
Layer；Again by graphene oxide/Fe3O4Graphene oxide reduction in aeroge, thus to obtain the stone for the layer structure that lamella stacks
Black alkene/Fe3O4Composite wave-suction material.
In the graphene/Fe3O4In composite wave-suction material, magnetic nanoparticle --- Fe3O4Uniform load is in graphene
The surface of carrier and lamella, not only density is light for the composite wave-suction material of formation, intensity is high, but also has both magnetic loss and electrical loss,
And dielectric constant is adjustable.Graphene/the Fe3O4The electromagnetic performance matching feature of composite wave-suction material absorbs it more
Rather than reflection electromagnetic wave, to reduce secondary pollution of the electromagnetic wave to environment.
Detailed description of the invention
Fig. 1 is graphene/Fe provided in an embodiment of the present invention3O4The photo of composite wave-suction material；
Fig. 2 is graphene/Fe provided in an embodiment of the present invention3O4The SEM of composite wave-suction material schemes, and wherein Fig. 2 a is surface
Shape appearance figure, Fig. 2 b are construction profile；
Fig. 3 a is provided in an embodiment of the present invention for graphene/Fe3O4The XRD diagram of composite wave-suction material, Fig. 3 b are graphite
Alkene/Fe3O4The Raman spectrogram of composite wave-suction material；
Fig. 4 is graphene/Fe of different-thickness provided in an embodiment of the present invention3O4The suction wave effect test knot of composite material
Fruit figure.
Specific embodiment
In order to make the objectives, technical solutions, and advantages of the present invention clearer, with reference to the accompanying drawings and embodiments, right
The present invention is further elaborated.It should be appreciated that the specific embodiments described herein are merely illustrative of the present invention, and
It is not used in the restriction present invention.
The embodiment of the invention provides a kind of graphene/ferroso-ferric oxide composite wave-suction material preparation methods, including with
Lower step:
Prepare graphene oxide dispersion, FeCl2Solution and FeCl3Solution；
Above-mentioned three kinds of liquid is mixed, is stirred 2-3 hours under 80-120 degree (preferably 100 degree), oxidation stone is obtained
Black alkene/Fe3O4Dispersion liquid；
By the graphene oxide/Fe3O4Dispersion liquid vacuum drying, obtains graphene oxide/Fe3O4Aeroge；
By the graphene oxide/Fe3O4Aeroge heating, obtains graphene/Fe3O4Aeroge, by the graphene/
Fe3O4Aeroge carries out Mechanical pressing, obtains graphene/Fe3O4Composite material；Graphene/the Fe3O4Composite material is lamella
The layer structure of stacking.
Graphene provided in an embodiment of the present invention/ferroso-ferric oxide composite wave-suction material preparation method, makes full use of oxygen
- OH is rich in graphite alkene, the functional groups such as-COOH can be used as nucleation site, react generation with iron ion and ferrous ion
Fe3O4.The preparation method first uses graphene oxide dispersion, FeCl2Solution and FeCl3Solution prepare graphene oxide/
Fe3O4Aeroge, Fe3O4Surface and lamella of the uniform load in graphene carrier；Again by graphene oxide/Fe3O4In aeroge
Graphene oxide reduction, thus to obtain lamella stack layer structure graphene/Fe3O4Composite wave-suction material.
In the graphene/Fe3O4In composite wave-suction material, magnetic nanoparticle --- Fe3O4Uniform load is in graphene
The surface of carrier and lamella, not only density is light for the composite wave-suction material of formation, intensity is high, but also has both magnetic loss and electrical loss,
And dielectric constant is adjustable.Graphene/the Fe3O4The electromagnetic performance matching feature of composite wave-suction material absorbs it more
Rather than reflection electromagnetic wave, to reduce secondary pollution of the electromagnetic wave to environment.
Specifically, the preparation process of the graphene oxide dispersion includes: that graphene oxide is soluble in water, at ultrasound
Manage 30-40min；The concentration of the graphene oxide dispersion is 0.1-10mg/ml, FeCl2The concentration of solution is 10-20mg/
Ml, FeCl3The concentration of solution is 20-30mg/ml.The graphene oxide dispersion, FeCl2Solution and FeCl3The volume of solution
Than for 5-10:1-3:2-4, preferably 6:1:2.
Graphene oxide/the Fe3O4Fe in dispersion liquid3O4Content is 10-50%.Fe3O4Content is too low, magnetic Nano
The wave-absorbing effect of particle is unobvious；Too high levels not only waste consumptive material, but also increase the weight of composite material.The Fe3O4Grain
Diameter is 20-60nm, the concentration and reaction time control that the partial size passes through iron ion and ferrous ion.The particle size can
To guarantee Fe3O4Equably it is supported on surface and the lamella of graphene carrier.
The vacuum drying temperature is 60-80 degree, and time 18-24h, 60 degree of preferable temperature, the time is for 24 hours.It is described to add
Hot temperature is 200-400 DEG C, and the time is 2-4 hours.By the way that the temperature and time of the heating is adjusted, control is obtained
Graphene/Fe3O4The density of aeroge.Graphene/the Fe3O4The density of aeroge is 0.1-1g/cm3。
Specifically, the graphene/Fe3O4Composite material with a thickness of 0.01-5 μm.
Graphene/the Fe3O4Composite material with a thickness of 1-2 μm, suction wave efficiency be 25-62dB.
The Mechanical pressing is by the graphene/Fe3O4Aeroge is placed in 10-20MPa, preferably carries out under 15MPa pressure
Mechanical pressing, the size by adjusting mechanical pressure can control graphene/Fe obtained3O4The thickness of composite material.
The embodiment of the invention also provides a kind of graphene/ferroso-ferric oxide composite wave-suction materials, using above-mentioned preparation
Method is made.
Fig. 1 is graphene/Fe of technical solution according to the invention preparation3O4The photo of composite wave-suction material, it is described compound
The different size of film of 1cm × 1cm to 10cm × 10cm can be made in absorbing material according to demand, can with a thickness of 0.01-5nm
It adjusts.
Fig. 2 is graphene/Fe3O4The SEM figure (electron scanning imaging figure) of composite wave-suction material, wherein Fig. 2 a is surface shape
Looks figure, Fig. 2 b are construction profile.From figure 2 it can be seen that graphene/the Fe3O4For the layer structure that lamella stacks, stone
Black alkene shows the pleated structure of gel, and ferroferric oxide nano granules are evenly distributed in the surface of graphene sheet layer.
Fig. 3 a is graphene/Fe3O4The XRD diagram (X-ray diffractogram) of composite wave-suction material, it can be seen from the figure that typical
Ferroso-ferric oxide characteristic peak can be observed out, and the not characteristic peak of graphene oxide illustrates graphene oxide
Thoroughly it has been reduced into graphene.Fig. 3 b is graphene/Fe3O4The Raman spectrogram of composite wave-suction material, from figure can from
To the raman characteristic peak of graphene.
Graphene paper/Fe of different-thickness prepared by technical solution according to the invention3O4Composite material carries out inhaling wave effect
It can test, as a result as shown in Figure 4.It can be seen from the figure that the composite wave-suction material under thin thickness (2mm), inhales wave effect
62dB can be can achieve.This in lightweight composite material be before it is unapproachable, composite material has the wide (2- of absorption band
18GHz), the good feature of wave efficiency is inhaled.
Graphene/Fe of preparation of the embodiment of the present invention3O4Composite wave-suction material have light weight, thickness is thin, intensity is high, inhale
The good feature of bandwidth, absorbing property is received, has in radome, Medical Devices, electronic equipment or even military field and widely answers
Use prospect.
Technical solution of the present invention is described in detail below in conjunction with specific embodiment.
Embodiment 1
The preparation of graphene oxide: graphene oxide is prepared using Hummer method, prepares graphene oxide after ultrasound removing
Dispersion liquid, concentration 0.8mg/ml；
Graphene paper/Fe3O4The preparation of composite wave-suction material:
0.4g graphene oxide powder is dissolved in 100ml water, ultrasonic 35min, supersonic frequency forms dense for 200-300Hz
Degree is the graphene oxide dispersion of 4mg/ml；
Weigh 0.4g FeCl2·4H2O is simultaneously dissolved in 20ml water, weighs 1g FeCl3·6H2O is simultaneously dissolved in 40ml water；
The above-mentioned solution prepared is added in the graphene oxide solution, is stirred 2.5 hours under 100 degree, is formed
Graphene oxide/Fe3O4Uniform dispersion liquid (wherein Fe3O4Content be 25%, Fe3O4Partial size be 30nm)；
By graphene oxide/Fe3O4Dispersion liquid is freeze-dried for 24 hours under vacuum, forms graphene oxide/Fe3O4Airsetting
Glue；
By graphene oxide/Fe3O4Aeroge heats 3 hours at 300 DEG C in electric furnace, forms graphene/Fe3O4Airsetting
(density of aeroge is 0.5g/cm to glue3)；
By graphene/Fe3O4Aeroge forms graphene paper/Fe in 15MPa mechanical pressure lower sheeting3O4Composite wave-absorbing material
Material.
Embodiment 2
The preparation of graphene oxide: graphene oxide is prepared using Hummer method, prepares graphene oxide after ultrasound removing
Dispersion liquid, concentration 7.5mg/ml；
Graphene paper/Fe3O4The preparation of composite wave-suction material:
0.4g graphene oxide powder is dissolved in 100ml water, ultrasonic 40min, supersonic frequency 200-300Hz, is formed
Concentration is the graphene oxide dispersion of 4mg/ml；
Weigh 0.4g FeCl2·4H2O is simultaneously dissolved in 20ml water, weighs 1g FeCl3·6H2O is simultaneously dissolved in 40ml water；
The above-mentioned solution prepared is added in the graphene oxide solution, is stirred 3 hours under 100 degree, oxygen is formed
Graphite alkene/Fe3O4Uniform dispersion liquid (wherein Fe3O4Content be 45%, Fe3O4Partial size be 45nm)；
By graphene oxide/Fe3O4Dispersion liquid is freeze-dried for 24 hours under vacuum, forms graphene oxide/Fe3O4Airsetting
Glue；
By graphene oxide/Fe3O4Aeroge heats 2.6 hours at 220 DEG C in electric furnace, forms graphene/Fe3O4Gas
(density of aeroge is 0.3g/cm to gel3)；
By graphene/Fe3O4Aeroge forms graphene paper/Fe in 15MPa mechanical pressure lower sheeting3O4Composite wave-absorbing material
Material.
The foregoing is merely illustrative of the preferred embodiments of the present invention, is not intended to limit the invention, all in essence of the invention
Made any modifications, equivalent replacements, and improvements etc., should all be included in the protection scope of the present invention within mind and principle.
Claims (7)
1. a kind of graphene/ferroso-ferric oxide composite wave-suction material preparation method, which comprises the following steps:
Prepare graphene oxide dispersion, FeCl2Solution and FeCl3Solution；
Above-mentioned three kinds of liquid is mixed, is stirred in 80-120 degree, graphene oxide/Fe is obtained3O4Dispersion liquid；
By the graphene oxide/Fe3O4Dispersion liquid vacuum drying, obtains graphene oxide/Fe3O4Aeroge；
By the graphene oxide/Fe3O4Aeroge heating, obtains graphene/Fe3O4Aeroge, by the graphene/Fe3O4
Aeroge carries out Mechanical pressing, obtains graphene/Fe3O4Composite material；Graphene/the Fe3O4Composite material is lamella stacking
Layer structure；
The preparation process of the graphene oxide dispersion includes: graphene oxide is soluble in water, ultrasonic treatment 30-40min；
The concentration of the graphene oxide dispersion is 0.1-10mg/ml, the FeCl2The concentration of solution is 10-20mg/ml, described
FeCl3The concentration of solution is 20-30mg/ml；
The graphene oxide dispersion, FeCl2Solution and FeCl3The volume ratio of solution is 5-10:1-3:2-4.
2. preparation method as described in claim 1, which is characterized in that the graphene oxide/Fe3O4Fe in dispersion liquid3O4
Content is 10-50%, the Fe3O4Partial size be 20-60nm.
3. preparation method as described in claim 1, which is characterized in that the vacuum drying temperature is 60-80 degree, and the time is
18-24h。
4. preparation method as described in claim 1, which is characterized in that the heating temperature is 200-400 DEG C, time 2-4
Hour.
5. preparation method as described in claim 1, which is characterized in that the graphene/Fe3O4The density of aeroge is 0.1-
1g/cm3。
6. preparation method as described in claim 1, which is characterized in that the graphene/Fe3O4Composite material with a thickness of
0.01-5nm。
7. preparation method as described in claim 1, which is characterized in that the graphene/Fe3O4Composite material with a thickness of 1-2
μm, suction wave efficiency is 25-62dB.
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| CN111592376B (en) * | 2020-06-08 | 2021-06-08 | 北京化工大学 | Preparation method of composite aerogel functional material based on ferroferric oxide nanowire/graphene oxide interpenetrating structure |
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Effective date of registration: 20210317 Address after: No.16, Keji Third Road, circular economy industrial park, Yongji economic and Technological Development Zone, Yongji City, Yuncheng City, Shanxi Province 044000 Patentee after: Shanxi Ganneng Semiconductor Technology Co.,Ltd. Address before: 518000 No. 3688 Nanhai Road, Shenzhen, Guangdong, Nanshan District Patentee before: SHENZHEN University |
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Effective date of registration: 20210927 Address after: 335400 in the park, No. 1, chemical Avenue, Huayuan street, Guixi City, Yingtan City, Jiangxi Province (the former site of Liuguo chemical industry) Patentee after: Guixi crossing Photoelectric Technology Co.,Ltd. Address before: No.16, Keji Third Road, circular economy industrial park, Yongji economic and Technological Development Zone, Yongji City, Yuncheng City, Shanxi Province 044000 Patentee before: Shanxi Ganneng Semiconductor Technology Co.,Ltd. |